참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfamic Acid | HCID 5987 | — |
| 반응물 | 2,5-Dichloroaniline | HCID 7262 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | N-[beta-(beta-ethoxy)ethoxy]ethyl-N-ethylaniline | HCID 21424342 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 반응물 | HCID 178526385 | HCID 178526385 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 54018568 | HCID 54018568 | — |
반응 단계
16.1 g (0.1 mole) of 2,5-dichloroaniline was dissolved in a mixed solution of 85 ml of concentrated hydrochloric acid and 200 ml of water while stirring with heating on a water bath and the solution was cooled to 5° C and a solution prepared by dissolving 8.28 g (0.12 mole) of sodium nitrite in 50 ml of water was slowly added dropwise. The temperature was kept at 5° C and after completion of the addition of the solution was stirred for 20 minutes, sulfamic acid was added thereto to decompose excess HNO2. Thereafter, the solution was filtered and added at a time to a solution prepared by dissolving 23.6 g (0.1 mole) of N-[β-(β-ethoxy)ethoxy]ethyl-N-ethylaniline in 1 l of 1N-HCl. Furthermore, about 500 ml of water was added thereto and with stirring about 200 g of sodium acetate were added thereto. After allowing to stand for several hours, it was filtered and the azo dye which adhered to wall of device and filter paper was collected and used for the next reaction without purification. The crude product was 34.1 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04035188 |
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| 출처 데이터셋 | uspto-grants-1977_07 |
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| ORD ID | ord-1710c168a65e4362bac6e98310e89f7b |
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| 출처 메모 | uspto-grants-1977_07 |
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